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Sodium Methoxide → {2-Methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 1-Benzoyl-3-{2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea | HCID 22015736 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | {2-Methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea | HCID 22015743 | 97% |
反応手順
To a stirred suspension of 2.00 g (5.36 mmol) 1-benzoyl-3-{2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea in 13 ml methanol was added dropwise 0.15 ml (0.80 mmol) 5.4 M sodium methylate solution and stirring continued for 1 h at room temperature. The mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Flash chromatography (ethyl acetate) afforded 1.40 g (97%) {2-methoxy-5-[(2-methoxy-ethyl)-methyl-amino]-phenyl}-thiourea as an amber oil. ES-MS m/e (%): 270 (M+H+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713499B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-1ea0648519114dda86f440fe12a9734a |
| 出典メモ | uspto-grants-2004_03 |